Process of producing nitrids.



C. E. ACKBR. PROCESS 0F PRODUGING NITEIDS. APPLICATION FILED MAR. Ia,1909.

Patented Dec. 14, 1909.

CHARLES E. ACKER, OF NEW YORK, N. Y., ASSIGNOR TO THE CORPORATION OF NEWYORK.

PROCESS 0F PRODUCING NITRIDS.

Specification of Letters Patent.

Patented Dec. 14, 1909.

\ Application Afiled March 18, 1909. Serial No. 484,187.

To all whom it may concern:

Be it known that I, CHARLES E. AcKnR, a citizen of the United States,residing at New York, in the county of New York and State of New York,have invented certain new and useful Improvements in Processes ofProducing Nitrids,of which the following is a specification.

This process relates to the electrolytic production of nitrids,especially those of the alkali and alkaline-earth` metals.

The preferred process comprises the steps of electrolyzing a moltencompound of the metal which is to be combined with nitrogen, alloyingthe separated metal with a-cathode metal, reacting on the alloyed metalwith a nitrogenous gas, and returning the residual metal to the cathode.Incidental steps are the injection of the nitrogenous gas in a directionto cause or assist the circulationy of the alloy and residual metal; andthe cooling of the alloy before treatment with the gas, especially bymaintaining opposed adjacent streams of the alloy and residual metal..Apparatus which may be used in carrying out the process is shown in theaccompany` ing drawings, in Which- Y Figures l, 2, 3 arevertical'l'ongitudinal sections of three different constructions, eachcomprising an electrolytic cell and a separate connected chamber fortreating the alloy.

Each apparatus illustrated has the l .eral construction of thatheretofore devised by me for the production of caustic alkali. theelectrolytic cell comprising a cast iron vessel l lined at the sideswith magnesia brick 2, inclosed in brickwork 3 and covered by arefractory slab 4, throughwhich pass the depending carbon anodes 5. Inthe bottom of the vessel is a shallow layer 6 of a molten heavy inertmetal such as lead, constituting the cathode, upon Which is the moltenelectrolyte 7. Theivessel 1 -is connected by delivery and return pipesor ducts 8, 9 to a separate chamber 10, into which the nitrogenous gasmay be introduced by a valved pipe 11. The chamber 10 may be inclosed inthe brickwork 3, as shown in Figs. 1, 3, or may be outside it as shownin Fig. 2, depending desired to maintain therein.

The delivery pipe 8 of the apparatus shown in Fig. 1 is provided with aseries of genon the temperature which it is annular heat-radiatingflanges 12, to cool the alloy therein. v The delivery pipe 82 of theapparatus shown in Fig. 2 has a lower portion which receives a.supplemental gas inlet pipe 13 and thence inclinesupward to the chamber10, the gas injected through the pipe 13 and the light compoundsproduced by the gas -rising and moving along the pipe, facilitating thereaction therein. In the apparatus of Fig. 3, a portion of the deliverypipe 83 is enlarged and receives the return pipe 93, so that heat may betransferred from the outflowing alloy to the returning residual metal.and metal may be effected either solely by the current of injected gas,as in the apparatus of Figs. 1, 3, or by a mechanical device, forexample the screw shown in Fig. 2, or by both. If desired, the alloy maybe cooled by injecting a regulated amount of a cooled and 4compressedgaseous reagent.

The reaction chamber l0 is of the general construction of that employedin mycaustic alkali apparatus, comprising a vertical cen- Thecirculation of the alloy NITROGEN COMPANY, A

tral pipe 14, which -receives the molten alloy and injected as. Thenitrid resulting from the reaction, eing usually lighter than theresidual metal, rises and collects as a floating layer, which may be runout through a suitable outlet 15, the metal returning to theelectrolytic cell to reconstitute the cathode.

A specific process which may be carried out is the production of calciumnitrid by the injection of nitrogen into an electrolytic calcium-leadalloy.

I claim:

1. The cyclic process-of producing nitrids, whichA consists inrepeatedly reacting with nitrogen on an alloy comprising an inert metaland a nitrid-forming metal, separating the resulting nitrid, andalloying more of the nitrid-forming metal with the residual l inertmetal.

2. The cyclic process of producing nitrids, which consists in repeatedlyreacting with nitrogen on a molten alloy comprising an inert metal and anitridorming metal, sepa` rating the resulting nitrid, and alloyin moreof the nitrid-forming metal with the residual inert metal.

3. 'The cyclic process of producing nitrids, Which consists inrepeatedly reacting with nitrogen on a molten alloy comprislng an inertmetal and a nitrid-forming metal, separating the resulting ntrid, andalloying more of the nitrid-lt'orming metal With the residual molteninert metal.

4. The cyclic process of producing nitrids, which consists in injectinga nitrogenous gas into a molten alloy comprising an inert metal and anitrid-forming metal, separating the resulting nitrid, and alloying moreot' the nitrid-forming metal with the residual metal for furthertreatment. l

5. The electrolytic process of producing nitrids, which consists inelectrolyzing a molten compound of'a nitrid-forming metal, alloying theseparated metal with an inert .cathode metal, reacting on the moltenalloy with nitrogen, separating the resulting nitrid, and ree'mployingthe residual' inert metal'in the cathode.

6. The electrolytio process of producing nitrids, which consists inelectrolyzing a molten compound of a nitrid-forming metal, alloying tlieseparated metal With an inert cathode metal, injecting a nitrogenous`gas into the molten alloy, separating the resulting nitrid, andremploying the inert residual metal in the cathode. y 7. The cyclicprocess of producing alkaline-earth metal nitrids, which consists inrepeatedlyreacting Withnitrogen on an alloy comprising an inert metalAand an alkalineearth metal, separating the resultant nitrid, andalloying more of the alkaline-earth metal with the residual inert metal.

.8. The cyclic process of producing calcium nitrid, which consists inrepeatedly reacting `with nitrogen on an alloy 'comprising an inertmetal and calcium, separating the resultantn1tr1d,'and alloying morecalcium with the residual inert metal.

In testimony whereof, I aiix my signature m presence of two witnesses.

CHARLES ACKER.- Titnesses i ROBERT HARRISON, SUSIE E. SAMrsoN..

